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journal homepage: http://ees.elsevier.com/CEMCON/default.asp

Experimentation and modelling

Luc Courard , Herv Dege, Anne Darimont

University of Lige, Department of Architecture, Geology, Environment and Constructions, Belgium

a r t i c l e

i n f o

Article history:

Received 1 August 2013

Accepted 9 June 2014

Available online 12 July 2014

Keywords:

Hydration (A)

Mechanical properties (C)

CaO (D)

Concrete (E)

Pop-out

a b s t r a c t

When nodules of lime are embedded into concrete, the expansion accompanying the transformation of CaO into

Ca(OH)2 induces stresses and strains in both the lime nodule and in the concrete matrix. The concrete cover

thickness, the diameter and the shape of the lime nodule as well as the mechanical characteristics of concrete

and lime are the key parameters inuencing the development of internal pressure and hence controlling the

risk of cracking or pop-out. In order to study the effect of lime into cementitious concretes, laboratory investigations and modelling have been performed and show that the minimum cover thickness necessary to avoid the

development of the pop-out phenomenon is estimated of the order of half the diameter of the inclusion. This

is coming from the observation that expansion happens inside the porosity of the hydrated lime Ca(OH)2:

ESEM and DRX analyses conrm the effect of connement in the development of crystals.

2014 Elsevier Ltd. All rights reserved.

1. Introduction

Lime has been used for a very long time in construction and buildings: Roman cement was already made of a part of lime while it

remained the only binder used until modern cement was designed

during XIXth century [1]. Lime is an industrial product obtained by

calcination of limestone in a lime kiln [2]. This is described as a bright

lime (Table 1), because of its high reactivity with water. The bulk density

of the limestones industrially used for the manufacture of lime usually

offers a lower density than calcite used for ornamental stones: porosity

maybe up to 30% [3]. Quick lime is very reactive with water and

hydrates are quickly formed [4]. Hydration process is accompanied by

a signicant proliferation (Table 1). The formation of Ca(OH)2 yields

in larger volume (expansive reaction). The ratio of volume change

from CaO particle to Ca(OH)2 is 33.1/16.8 2.

The doubling of the molar volume (from 16.8 to 33.1 cm3/mol) is responsible for expansion during hydration [4]. The intensity and speed of

hydration are governed by lime purity, particle size, surface area, etc.

[5]. Burning temperature and kiln technology are also two important

discriminant factors in the case of industrial lime production [3].

An interesting parameter used to quantify the reactivity of lime is

the so-called T60, which is measured in accordance with standardized

method EN 459-2:2001. It gives the speed of lime extinction, or the

Corresponding author at: University of Lige, Civil and Mechanical Engineering

Institute (B 52/3). Chemin des Chevreuils, 1, B-4000 LIEGE, Belgium. Tel.:+32 4 366 93

50; fax: +32 4 366 92 38.

E-mail address: Luc.Courard@ulg.ac.be (L. Courard).

http://dx.doi.org/10.1016/j.cemconres.2014.06.005

0008-8846/ 2014 Elsevier Ltd. All rights reserved.

more reactive the lime is. In some cases, the lime can be dead burned,

leading to high density CaO grains [4]. This dead burn lime hydrates

very slowly because of a reduced porosity [6]. When lime is incorporated into concrete, problems due to expansion may occur (Fig. 1): this

phenomenon is well known as pop-out [711].

In many cases, quick lime is present in steel or iron slags [8,9]. That

means that it is rarely in the form of millimetre-sized aggregate in a conned environment. In the case of steel slags, Deng et al. [10] observed

that expansion rates are depending on the type of cement and the percentage of lime: for lime contents of 2 and 5% (by weight of cement), the

maximum observed rate of expansion is 0.12 and 0.7%, respectively, for

cement type CEM I. The expansion force is estimated at 11.87 MPa in

3 days. A dead lime was used for experimentation and required alkali

activation: the concentration of OH-ions in the pore solution of cement

paste controls the expansion by affecting the positions occupied by the

crystals of Ca(OH)2 and the pressure of crystallization. Analyses of the

behaviour of LD steel slags containing lime nodules [11] were also conducted as a result of damage observed. An expansion rate of 0.16%

(measured by immersion according to the Korean standard KS F 2580)

was considered. The nite element calculations show that the depth of

the pop-out increases as concrete strength decreases and the diameter

of the slag increases (Fig. 2).

Other authors [12,13] made investigations on ne lime particle coming from shrinkage preventing agents or wrong cement manufacturing.

Useful information may be found through the study of other

expanding processes [14]: Alkali Aggregate Reaction (AAR) should induce similar stresses inside concrete. A difference is however coming

74

Table 1

Hydration of quick to hydrated lime [2,3].

Property

CaO

+H2O

Ca(OH)2

Molecular weight

Bulk density (g/cm3)

Specic density (g/cm3)

Molar volume (cm3/mol)

56.08

1.401.90

3.33

56.08/3.33 = 16.8

18.01

74.09

0.450.65

2.24

74.09/2.24 = 33.1

from the easier fullling of aggregate cracks by the silica gel which

progressively replaces a part of the initial products present along the

edge of stone material.

With regard to the very poor information coming from literature

reviewing, it clearly appears a lack of knowledge on the behaviour of

quick lime aggregates (up to 20 mm diameter) when mixed into

concrete. A risk evaluation analysis is needed: it will be based on an experimental programme and modelling that will help in understanding

free lime behaviour in conned situation.

Fig. 2. Concrete cover versus diameter of the slag for different concrete types (from [11]).

concrete [16]. Bolomey formula also suggests a linear relationship

between the compressive strength and the ratio C/W.

f c;cube k

As a rst simplied preliminary approach, it is considered that the

swelling pressure is unable to induce cracking in the concrete as a

nodule of lime can merely be considered as an air bubble, whose effect

is increasing the porosity and, consequently, decreasing the compressive strength of concrete. Bolomey and Feret theories can be used to

quantify this phenomenon [15].

Based on the equation p (aggregates) + s (sand) + c (cement) + w

(water) + v (voids) = 1, which expresses the sum of the volume fractions for 1 m3 of concrete, we have, with = (c/(c + w + v)), the Feret

formula which expresses the relationship between the compressive

strength of concrete and the voids (v):

2

f c;cube K0 K0

2

c

with K0 K Rc

cwv

coefcient and Rc = the compressive strength of cement measured on

standardized mortar (EN 196-1).

This clearly indicates that the compressive strength decreases when

the w/c ratio increases. If we express this equation as a function of W

and C (mass ratio) for a cement relative density of 3.15, the expression

can be written:

1

f c;cube K0

2 :

1 3:15 CW

V

1cm

C

h1

W

cement, the age of the concrete, the shape and dimensions of the test

pieces, the curing conditions and the sieving curve of aggregates and

sand.

The volume occupied by the nodules can be considered as an additional volume of water in the sense of increasing W/C ratio; that will

partially produce an additional volume of air after curing and evaporation. If we consider for example a W/C = 0.5 and a bulk density of

lime 1.56 [3], the volume occupied by the nodules, for a percentage of

0.3% of the mass of aggregates into concrete (1300 kg/m3 of concrete),

would be: 0.003 1300/1560 = 0.0025 m3 = 2.5 l. This means that

we can consider a ctitious increase of the amount of water for a

350 kg concrete cement of about 2.5 l, which means a total of

175 + 2.5 = 177.5 l. The W/C ratio increases thus from 0.50 to 0.507.

Feret formula allows estimating the resulting loss of strength [16]:

1

1 3:15 0:502

1

1:017:

1 3:15 0:512

This evaluation clearly shows that the inuence of nodules inside the

concrete has a very marginal impact on the major structural characteristic of concrete: compressive strength is only lightly affected by a

reasonable level of pollution by lime nodules.

However, if these nodules are close to the surface, they are likely

to induce pop-out and cracking, which is detrimental for concrete

2cm

75

much slower to react because these are more compact than the type

of lime considered here.

Specic theoretical developments have thus been carried out to

assess the risk of such phenomena. Cracking and the emergence of a

burst are indeed conditioned by a number of factors related to the

materials:

the diameter of the nodule,

the concentration of nodules,

the conditions of connement of the nodule of lime (rate of

expansion, swelling pressure),

tensile strength of the concrete,

modulus of rigidity of lime (and hydrated lime) and concrete.

models are based on the mechanics of materials and on the theory of

elasticity. The study also assesses the sensitivity of the mechanical effects with respect to the various relevant physical parameters. Two congurations are studied. The rst one considers a nodule embedded

within the concrete mass: the objectives are in this case to estimate

the inuence zone of the nodule and the possible risks of interaction between neighbouring nodules, as well as the risk of crushing or cracking

of the concrete in the vicinity of the nodule. The second situation is

considering a nodule located near the free surface of the concrete,

with the main objective of evaluating the risk of occurrence of a popout phenomenon.

structure durability [17]. Only few data are available on this subject in

the literature [10,12,18] and mainly deals with the effect of the nodules

of lime in steel slag, most often used as aggregates for making concrete

Model 1 used in this situation considers a spherical nodule in perfect

contact with an environment encompassing innite dimensions. Both

76

media are assumed to exhibit an elastic behaviour. Although both materials are known to be largely inelastic, this model is however appropriate for low level of stresses and in particular to estimate the initiation

of cracking and can also provide a good understanding of the physical

phenomena with a limited computational effort.

Model 1 (Fig. 3) is based on the assumption that the swelling of the

nodule is partially prevented by pressure developing at the interface

between concrete and lime and conning the nodule. This pressure depends on the mechanical properties (elastic modulus and Poisson's

ratio) of the two materials, as well as on the amplitude of the swelling

as it would be observed if the nodule was perfectly free to expand

upon hydration. Assuming a spherical symmetry of the problem and a

perfect compatibility of the displacements at the interface between

lime nodule and concrete matrix, the pressure can be calculated using

Eq. (3), on the base of the relations proposed in [19] for spherical

containers under internal or external uniform pressure:

R

R

p

CL CC

with

CL

1 2L

EL

D=2

r p

3

D

2z

and

12C

EC

s

3 Vfinal

1:

Vinitial

3

p D=2

D

3 :

2 z

where EL and EC are the elastic modulus of hydrated lime and concrete,

respectively; L and C are the Poisson's ratio of hydrated lime and

concrete, respectively; R is the initial radius of the nodule and R is

the variation of the radius of the nodule due to hydration process.

R/R ratio can be directly related to volume variation by means of

Eq. (6):

R

is needed to distinguish compressive stresses r, acting in radial direction, and tensile stresses t, oriented in the circumferential direction.

They are given in Eqs. (7) and (8), respectively:

3

and

CC

developed, it is possible to calculate the stress distribution in the

in compression. Furthermore, D is the diameter of the inclusion and z

is the distance from the interface concrete/inclusion to the considered

point inside the concrete.

These stresses can then be compared to the compressive and tensile

strength of the concrete in order to assess the risk of a local crushing

around the nodule or of occurrence of radial cracks associated with

circumferential tension in the vicinity of the nodule. On the other

hand, the model allows estimating the area of concrete mechanically

disturbed by the presence of a swelling nodule.

2.2.2. Effect of a nodule in the vicinity of the concrete surface

A second model (Fig. 4) is used to assess the risk of local bursting of

concrete (pop-out). It is now assumed that the swelling pressure is no

more balanced by a stress distribution with spherical symmetry, but

rather by a tensile stress distribution varying linearly from the inclusion

towards the surface and distributed on a truncated cone.

Based on this failure pattern, one can evaluate the maximum tensile

stress acting at the base of the truncated cone with the following

equation:

2

pR

#

t "

2

R e

RR e

tg

3tg2

where R is the radius of the nodule, p is the pressure induced at the interface between nodule and concrete, e is the thickness of concrete

Table 2

Evaluation of the contact pressure vs lime and concrete properties.

Cellular concrete block C4

Concrete

EC

(MPa)

R/Rmean

(%)

R/Rmax

(%)

Pmean

(MPa)

Pmax

(MPa)

2000

4000

15,000

22

16

7

24

19

12

32

24

11

35

29

19

covering and is the angle of the ejection cone with respect to the concrete surface. Eq. (9) simply translates the fact that the resultant of

swelling pressure acting on the bottom part of the nodule is directly balanced by the vertical resultant of tensile stresses acting at the surface of

the ejection cone and that the pop-out effect is initiated when the local

tension stresses exceed the tension resistance of the concrete matrix.

Based on the evaluation of the swelling pressure obtained from

model 1, tensile stress can be calculated from model 2 and compared

to the tensile strength of concrete to assess the risk of pop-out.

Table 3

Evaluation of the contact pressure vs E modulus of lime (EL) and concrete (EC) and volume

(radius) variation of lime.

EL

(MPa)

V/V

(%)

R/R

(%)

p [EC = 7000]

(MPa)

p [EC = 15,000]

(MPa)

p [EC = 30,000]

(MPa)

100

10

20

30

40

50

10

20

30

40

50

10

20

30

40

50

3

6

9

12

14

3

6

9

12

14

3

6

9

12

14

6

12

18

23

28

9

18

27

35

42

12

24

35

46

56

6

12

18

24

29

10

19

27

35

43

13

25

36

47

57

6

12

18

24

29

10

19

27

35

43

13

25

36

47

57

150

The objectives of the experimental investigations and analyses

were:

to quantify expansion rate of lime,

to characterize the quality of hydrated lime (densication process),

to select data for calculation modelling (expansion and compressibility

modulus of free lime).

Free lime (from 80 to 120 mm limestone blocks) is representative

of a production process with a classical reactivity (T60 = 2 min 17 s)

and purity; density is equal to 1.44 g/cm3. Samples ( = 18.5 mm

and H = 15 to 20 mm) are cored in the lump lime. Concrete blocks

of 190 190 85 mm3 have been rstly used to simulate conning

effect. They provide a compressive strength of 15 N/mm2 and a density

of 2.2 g/cm3. This type of porous concrete has been selected in order to

favour water transmission and lime reaction.

3.2. Conning operations

A cylindrical opening of 19 mm diameter (Fig. 5a) and 25 mm deep

(Fig. 5b) is cored in the blocks by means of a drill. To study the impact of

the situation of the nodule of lime from the concrete surface, the holes

are made at different distances from the edge of the concrete block

(Fig. 5c). To ensure the best connement possible, nishing cylindrical

orices are performed with quick-setting cement to ll the cone left

by the bit, to smooth the cylinder walls and to repair the damaged

edge of the whole drilling. However, despite these precautions, connement is not perfect: the top surface of the block is not perfectly at and a

77

200

(Fig. 5d).

The connement of the concrete block is then ensured by steel plates

and clamps. A plastic sheet is inserted under the steel plate for

preventing any reaction between lime and steel (Fig. 6). The assembly

is then immersed in water and the water level is adjusted under the

top edge of the block (Fig. 7).

A reference test is made in order to check the time needed for a

complete hydration of a free lime cylinder: it was measured that

67 hour storage into water allowed a full hydration of the sample by

means of water transfer through the porosity of the sample.

The blocks are then cut with a diamond saw (dry) at the right and

the edge of the nodule, in order to observe possible internal cracks. Hydrated lime cores are then recovered, measured, weighed and analyzed

on the base of the loss on ignition at 100 C (moisture measurement)

and 600 C (measuring the rate of hydration).

3.3. X Ray Diffraction and microscopical analysis

X Ray Diffraction analyses have been carried out in order to determine

the mineralogy of the crystals and the nature of the hydrated products.

Samples observed with Environmental Scanning Electron Microscope

(ESEM) are similar to the one used for XRD investigations. The samples

are glued on metal pads using a conductive adhesive. The specimens are

78

thus metallized with Pt before being introduced into the vacuum chamber

of a scanning electron microscope ESEM. The electron beam gives a view

of topography and shape of hydrated lime. EDAX (Philips) system,

coupled with ESEM, allows the detection of elements identied on a

spectrum according to their energy dispersion.

These analyses allow obtaining a good identication of different

forms of calcium hydroxide crystals under connement.

4. Results and discussions

4.1. Stress calculation and modelling hypothesis

In order to feed the proposed models, data needed are:

Elastic modulus of hydrated lime and concrete,

Poisson's ratio of hydrated lime and concrete,

Variation of volume of nodule during hydration.

The elastic modulus and Poisson's ratio of lime are estimated from

[20]: the value used for the elastic modulus of 100 MPa and Poisson's

ratio is 0.25. Results obtained from the experimental programme running

(chapter 4). The module of the concrete is of the order of 30 GPa and its

Poisson's ratio is considered equal to 0.2. It will be shown later on that

the results are quite insensitive to these latter values.

The swelling rate is more difcult to estimate. In fact, if the volume

variation of the lime during hydration can reach values as high as

200%, these values are only relevant in the absence of any connement.

The tests carried out in the framework of the present study show indeed

that the volume variation signicantly depends on the stiffness and

strength of the conning medium. The results presented in chapter 4

and other tests on lightweight concrete blocks show that, if one measures the change in diameter of cylindrical samples in the direction of

connement (i.e. in the radial direction) for samples with a diameter

which is adjusted to the initial hole made in the conning medium,

and which therefore are in contact with this medium from the start of

the hydration reaction, the average value of R/R is:

22% for connement in cellular concrete block of 2 MPa compression

characteristic strength,

16% for connement in cellular concrete block of 4 MPa compression

characteristic strength,

Fig. 10. Evolution of tensile stresses vs contact pressure and nodule diameter.

Table 4

Thickness of the potentially cracked zone around nodule of D diameter vs tensile strength.

V/V

(%)

(MPa)

(MPa)

(MPa)

10

20

30

40

50

0.19 D

0.36 D

0.48 D

0.57 D

0.64 D

0.11 D

0.26 D

0.37 D

0.45 D

0.51 D

0.07 D

0.21 D

0.30 D

0.37 D

0.43 D

characteristic strength.

These values correspond to respective volume variations (V/V) of

49, 34 and 15%, respectively.

This observation is explained by the fact that, when the conning

pressure reaches a sufcient level, it forces the hydration reaction to

occur towards the inside of the lime sample. This reaction proceeds

thus at constant volume and pressure, but results in a more dense

hydrated material. It is therefore expected that its elastic modulus be

higher than the reference value of 100 MPa.

Eqs. (7), (8) and (9) cannot be directly applied in the purpose of

comparison with the case of cylindrical test samples: the above

equations indeed assume a spherical inclusion. The transition to the

cylindrical case, however, can be done quite simply by changing the

coefcients Cb and Cch:

12L 1 L

CL

EL

10

and

CC

1 C

:

EC

11

pressure developed for the different test conditions (Table 2).

79

One might conclude from the values in Table 2 that the pressure required to conne the reaction varies with the material. It must however

be noted that the model assumes an elastic behaviour of the conning

material whatever the value of the pressure, while an evaluation of

the stresses developed in the conning medium for the cellular concrete

block case (i.e. c,max = p and t,max = p/2) concludes that they exceed

by far the resistance of the blocks. Calculations show that, for a sample

of 18 mm diameter, the resistance is actually exceeded on a thickness

approximately equal to the diameter of the sample. It can therefore be

estimated that the effective stiffness of the zone of the conning

medium directly surrounding the inclusion is reduced with respect to

its reference undamaged value, thereby increasing the value of the

coefcient CC and reducing consequently the pressure so as to reach a

balanced situation between effective stiffness and pressure. A rened

modelling of this phenomenon would however require advanced tools

that are considered out of the scope of the present study. One must

also note that cracks were indeed observed in the zone surrounding

the inclusion for some of the cellular concrete blocks used for connement tests, which is in accordance with the above conclusions. On the

other hand, for an ordinary concrete containment, the calculated level

of pressure is such that the stress remains at a level below the resistance

of the material. The model reproduces thus correctly the experimental

trends.

The range of parameters considered for the upcoming parameter

studies is dened by:

EC: 7000, 15,000 and 30,000 MPa, which corresponds to concrete

connement ranging from poor characteristics to ordinary

concrete;

EL: 100 to 200 MPa, ranging from a normal value to a value doubled

to take into account densication of lime during hydration. Experimental tests shows actually that, for the samples corresponding to

hydration in heavy concrete blocks, and thus with the highest

densication rate, the value of the measured elastic modulus is

about 150 MPa;

L and C are equal to 0.25 and 0.20 (values from the technical

literature), respectively;

Change in volume of the spherical inclusion varying from 10 to

50%, which corresponds to changes in radius of 3 to 15%, respectively. This range roughly sweeps the radius variation observed

Fig. 11. Evolution of the minimal thickness of concrete cover vs nodule diameter (minimum pressure).

80

Fig. 12. Evolution of the minimal thickness of concrete cover vs nodule diameter (mean pressure).

(observed values varying between 3 and 12%).

Finally, it must be stated that, as illustrated in Fig. 8, the pressure

level provided by the model for a given volume variation (Pn,model) is

obviously an upper bound of the actual value (Pn,actual) due to the

following reasons:

The model assumes that the inclusion and the conning materials are

in perfect contact and exhibit a spherical symmetry, while they

actually very often show signicant shape irregularities. In order to

provide order of magnitudes, it is relevant to note that, for same

volume variation and initial diameter, the pressure calculated for a

cylindrical inclusion is 25% less than the one calculated for a spherical

inclusion (i.e. the slope of the real pressure vs volume curve is

lower than the one given by Eqs. (3) and (6));

The model assumes that the contact is established from the beginning

of swelling. In reality, it can be assumed that a part of the measured

volume variation (V0) is corresponding to the lling of the voids

between the inclusion and the matrix; the real pressure should

therefore be associated with only a fraction of the volume change;

The model assumes that the elastic modulus of lime is constant

throughout the swelling phase, whereas it is in fact a phenomenon

whose parameters vary with time. The mechanical characteristics of

hydrated lime at the initiation of the swelling (ini) are corresponding

to an unconned environment and progressively evolve to those of

hydrated lime properties in conned environment (fin). The model

conservatively considers the stiffer situation (fin) throughout the

entire swelling process.

The level of conservatism of the chosen modelling assumptions is

however quite impossible to quantify.

4.2. Model exploitation and parametric study

4.2.1. Evaluation of the contact pressure

Results of the calculation of the contact pressure are presented on

Table 3. It is showed that pressure is roughly independent from the

Fig. 13. Evolution of the minimal thickness of concrete cover vs nodule diameter (maximum pressure).

Table 5

Hydrated lime content of the samples.

Test

[%]

Ca(OH)2 content

[%]

8

9

12

17

24.2

23.9

23.6

23.7

99.6

98.1

96.9

97.4

quality of concrete. However, results are clearly inuenced by the rigidity of the lime and the variation of the volume: estimated pressure

ranges from 6 to 57 MPa (this latter value is clearly unrealistic but

denes an absolute upper bound that would never be overtaken even

for the worst conditions). It has also to be mentioned that a possible variation of the Poisson's ratio of the lime could induce signicant variation

81

of the pressure: e.g. for an elastic modulus equal to 100 MPa, a variation

of volume corresponding to 30% and Poisson's ratio equal to 0.2, 0.25

and 0.3, resulting pressure is equal to 15, 18 and 23 MPa respectively.

For the reasonable average values of the parameters (EL = 150 MPa

and volume variation of 20%), pressure is up to 19 MPa, which is however

a clearly conservative estimate of the real pressure, as illustrated on Fig. 8.

4.2.2. Stress distribution

Compressive and tensile stress distributions are given in Figs. 9 and

10 for several values of pressures and nodule diameters. Curves are

corresponding to 3 levels of pressure taken from Table 3:

Pmin = 6 MPa (pressure calculated on the base of minimalistic

hypotheses),

Pmean = 19 MPa (pressure conservatively calculated on the base of

most probable hypotheses),

(e) Free lime nodule at 5 mm depth : pop out but no internal crack

Fig. 14. Sections of concrete blocks and free lime nodules.

82

(a)

(b)

Fig. 15. Free lime nodule at 5 mm depth (a) and 10 mm depth (b).

extreme hypotheses).

Values of stresses are calculated for 3 lime nodule diameters: 2, 10

and 20 mm, respectively. On Fig. 9 providing tensile stresses, horizontal

straight line corresponds to the mean tensile strength of ordinary

C25/30 concrete.

The gure related to compressive stresses (Fig. 9) shows that,

around a nodule which is assumed to be perfectly smooth and spherical, the stress level is equal to the pressure. For extreme conditions,

this level is likely to exceed the level of resistance of ordinary concrete. However, for average conditions, this level remains acceptable.

The curves also clearly show that the stress level rapidly decreases

with the distance from the nodule. Consequently, at a distance

equal to two times the diameter, the stress level is only about 1% of

the pressure and goes down to less than 0.1% at a distance

corresponding to 5 times the diameter. It can therefore be concluded

that:

Local crushing of the concrete near the nodule is normally not to be

feared;

The area of inuence of a nodule is of the order of 2 to 3 times the diameter (measured from the centre of the nodule). Assuming that the

minimum distances between nodules are in the order of 100 mm, the

areas potentially impacted by the presence of nodules are unlikely to

interfere.

Fig. 10 shows that, except for the minimum conditions, there exists a

region around the nodule where tensile forces are potentially present

and thus likely to initiate micro-cracking. No signicant cracking has

however been observed in tests performed in the laboratory for lime hydration in heavy concrete blocks (chapter 4). Table 4 gives the thickness

of the potentially cracked area corresponding to a module of lime E =

150 MPa for different values of the volume change and of the tensile

strength of the concrete (corresponding to percentiles of 5, 50 and 95,

respectively, for standard concrete C25/30).

One must be reminded that the values of radial swelling measured

in the laboratory (chapter 4) are of the order of 7% (so corresponding

to a volume variation V/V about 15%). However, in the worst case

(V/V = 50%) and for a very low concrete tensile strength (1.8 MPa),

the thickness of the cracked area is potentially of the order of 64% of

the diameter. Under these conditions, if these cracked zones are fully assimilated to non-resistant inclusions with a diameter equivalent to 2.28

times the diameter of the nodule (i.e. 1 D + 2 0.64 D), the calculation

of the effect of voids on the compressive strength of concrete according

to Section 1 of the present paper shows that, even in the case of cracking

around all the nodules included in the concrete (for a reasonable concentration of such lime nodules), the overall strength of the concrete

would hardly be affected.

4.2.3. Pop-out risk estimation

Figs. 11, 12 and 13 represent the results obtained by using the Eq. (9)

to estimate the risk of pop-out. These gures actually represent the

Table 6

Measurements of conned lime cylinders in concrete blocks (D is the distance between the nodule and the surface and d is the diameter of the nodule).

Test

Maximal connement

Restricted connement

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

Initial lime

Observations

Characteristics of hydrate

Density

(g/cm3)

D/d

Pop-out

(Y/N)

Cracking

(Y/N)

Density

(g/cm3)

Volume expansion

(%)

Radial expansion

(%)

Longitudinal expansion

(%)

1.38

1.58

1.44

1.44

1.38

1.49

1.47

1.39

1.43

1.40

1.41

1.46

1.50

1.39

1.45

1.51

1.41

1.50

4.5

4.5

4.5

4.5

4.5

4.5

2

2

1

1

1

0.5

0.5

0.5

0.25

0.25

2

0.25

N

N

N

N

N

N

N

N

N

N

N

Y

N

N

Y

Y

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

N

1.39

1.71

1.62

1.67

1.47

1.54

1.66

1.50

1.49

1.55

1.52

Unrecovered

1.50

1.46

Unrecovered

Unrecovered

1.14

1.31

32

22

18

14

24

28

17

23

27

20

23

10

5

7

3

6

8

8

6

8

8

6

8

11

4

6

11

9

1

8

8

3

9

32

25

12

7

5

10

64

51

24

27

76

73

83

1.84

Fig. 16. Evolution of the density of hydrated lime vs volume expansion (conned (tests 1 to 16) and less conned (tests 17 and 18)).

model predicts no occurrence of pop-out. This thickness is plotted as a

function of the diameter of the inclusion for different values of the

tensile strength of concrete and of the swelling pressure of the nodule.

The ejection angle is chosen equal to 30 in accordance with common

observations made on site. For facilitating the reading of the charts, a

light grey dash line outlines the situation where concrete thickness

equals the diameter of the nodule.

The following observations can be drawn from the analysis of these

gures:

For the minimal assumptions (low elastic modulus of the lime and

low ination rate Fig. 11), the risk of pop-out is almost negligible.

The model predicts occurrence of pop-out only for very low quality

of concrete (fct equal to 1.8 MPa). For higher values of fct, the estimated risk of pop-out is zero whatever the cover thickness, as shown on

Fig. 11 by perfectly horizontal superimposed lines corresponding to

fct equal to 2.6, 3.3 and 5.0 MPa. Even in the worst case, a cover

thickness less than 10% of the diameter appears sufcient to prevent

pop-out;

For the most realistic though conservative assumptions (intermediate

modulus of the lime and swelling ratio of 20% in volume Fig. 12), the

risk of pop-out is more important. For a tensile strength corresponding to ordinary concrete (2.6 MPa), the risk of pop-out occurs if the

thickness of the covering is of the order of half of the diameter (50%)

of the inclusion. This is to be compared with hydration tests on

Table 7

Rigidity modulus and compressive strength of hydrated lime cylinders (MPa).

Specimen reference

a

13 centred

14 centredb

17 centred

2C20

4C10

5C40

10C10

a

b

Non parallel faces.

Compressive strength

[MPa]

Rigidity modulus

[MPa]

5.1

5.1

5.4

8.3

3.8

5.3

5.4

150

164

189

168

129

180

144

for which pop-outs have been observed only for cover thicknesses of

10 and 5 mm (i.e. 50 and 25% of the diameter). Modelling and

observations seem to provide convergent results, conrming thus

the assumptions made on the different parameters entering in the

modelling process;

For extreme cases (Fig. 13), the model predicts ejection of pop-outs

for thicknesses of less than 1 to 2 times the diameter, according to

tensile strength of the concrete.

4.3. Conned free lime hydration results

4.3.1. Results of the tests

Eighteen trials were conducted, including 16 in the form of maximum connement (tests 1 to 16) and two under restricted connement

(tests 17 and 18), leaving more place for the hydrate to crystallize: the

connement is in fact restricted if the carrot of lime is of a size smaller

than the hole in the concrete. In this case, the metal plate is not

completely in contact with the concrete surface and allows some expansion of the lime. Several distances D from the edge of the concrete

substrate were tested: 4.5 to 0.25 times the initial diameter d of the

core of lime, respectively D/d in Table 6.

After testing conditions 8, 9, 13 and 17, respectively, loss of ignition

at 600 C was measured in order to evaluate the rate of hydration of the

lime (Table 5).

A minimum value of 97% of Ca(OH)2 is measured. If we consider that

initial lime is not totally pure it means less than 100% CaO due to

unburn limestone we may conclude that all the free lime has been

hydrated.

4.3.2. Internal cracking of the concrete blocks and pop-outs

No cracking has been observed for all the concrete blocks tested

(Fig. 14 a to e). Even for free lime nodules very close to the concrete surface (0.5 times free lime nodule diameter), no cracking appeared inside

the block.

Pop-outs were observed only for specimens (Fig. 15a and b) corresponding to depths:

0.25 times free lime nodule diameter (2 by 3 of the specimens) and

0.5 times free lime nodule diameter (1 by 3 of the specimens).

84

Lin (Counts)

Portlandite

220

210

200

190

180

170

160

150

140

130

120

110

100

90

80

70

60

50

40

30

20

10

0

NC1

d=2.62351

Portlandite

d=4.89551

Portlandite

d=3.10515

d=23.80000

d=26.83630d=16.23526

10

20

30

40

2-Theta - Scale

NC1 - File: NC1.raw - Type: 2Th/Th locked - Start: 2.000 - End: 45.000 - Step: 0.020 - Step time: 0.6 s - Temp.: 25 C (Room) - Time Started: 8 s - 2-Theta: 2.000 - Theta: 1.000 - Chi: 0.00 - Phi: 0.00 - X: 0.0

Operations: Background 0.000,0.000 | Smooth 0.150 | Import

04-0733 (I) - Portlandite, syn - Ca(OH)2 - Y: 86.46 % - d x by: 1. - WL: 1.5406 - 0 - I/Ic PDF 1.4 -

When depth was higher than 1 times the free lime nodule diameter,

no pop-out was observed.

4.3.3. Analysis of densication phenomenon and nodule expansion

As described in 3.2, the blocks are cut with a diamond saw (dry) at

the right and the edge of the nodule and hydrated lime cores are then

recovered, measured and weighed. As a reminder, in unconned

conditions, when quicklime CaO (bulk density about 1.5 g/cm3) is

transformed into Ca(OH)2 hydrate, it is in the shape of a powder of

low density (about 0.5 g/cm3). The measurements show (Table 6), in

conned situation, a densication process of the hydrate which

offers a density much higher than in unconned case. During these

tests, the hydrates obtained in conned environment showed a density

varying from 1.4 to 1.7 g/cm3, with an average value of 1.55 g/cm3

(Table 6).

This densication process logically implies a volume expansion

factor much lower than what is generally known when unconned

(300% as calculated from the ratio of 1.5 g/cm3 for lime divided by

0.5 g/cm3 for Ca(OH)2 hydrated lime). Expansion factors measured

here are in the range from 15 to 30% (23% average). Fig. 16 shows the

experimental values in the case of a high conned situation (tests 1 to

16, rhomb dots) and in the case of a partial connement (tests 17 and

18, square dots).

The positive expansion that is observed in the case of conned

samples (rhumb dots) means that these connements are not perfect,

leaving a free space for expansion. This imprecision is statistically distributed across different samples. These expansions are not related to

a deformation of the concrete block. It is possible to estimate the density

of the core hydrate in the case of perfect connement by extrapolating

the regression line. This extrapolation (82% correlation) allows to

calculate that, in the case of perfect connement (no volume expansion), the hydrate, formed from lime industrial bulk with a density of

1.5 g/cm3, will have an equivalent density of 1.84 g/cm3: this remains

less than the absolute density of the hydrate (2.2 g/cm3).

85

environment, leads to the production of completely hydrated portlandite

nodules with very high densities.

Some values from 100 to 200 MPa are given in the literature [19].

Due to the intrinsic variability of the free lime, tests have been performed on cylinder used for testing connement effect. Samples are

prepared exactly in the same conditions than in 3.2: after 67 hour

hydration, the cylinders are cored from concrete blocks (20 mm and

H1520 mm). Until testing, specimens are stored into plastic bags in

order to avoid carbonation process. Compressive loading is applied at

a speed of 5 N/s on an Instron 5585 tensile machine (Table 7).

These indicative measurements conrm literature results and have

been used as reference values for modelling (chapter 3).

portlandite type Ca(OH)2. Calcite can be present in very few quantities,

due to carbonation.

4.3.6. ESEM observations

The EDAX analysis conrmed the XRD analysis with bands, next to

oxygen and platinum bands, characterized by the presence of Ca.

4.3.7. NC1 sample

The unconned sample is in the form of powder, hard to stick on the

pad and difcult to be metallized. The porosity (Fig. 18(a)) is very high.

The grains are generally anhedral, rarely euhedral. They have a size

of 1 to 5 m (Fig. 18(b)).

X Ray Diffraction analyses have been carried out in order to determine the mineralogy of the crystals and the nature of the hydrated

products. Several samples have been recorded:

The sample shows expansion cracks (Fig. 19(a)). As in the periphery

than in the centre of the sample, small euhedral crystals are observed;

they attest that there was free space for them for growing and adopting

their own crystalline form. The crystals are associated with very small

needles blooms (Fig. 19(b)). The size of portlandite crystals ranges

from 0.1 to 5 m.

C110: 10 mm sample conned into concrete hole of 20 mm

diameter (75% Vf)

C115: 15 mm sample conned into concrete hole of 20 mm

diameter (44% Vf)

C120: 20 mm sample conned into concrete hole of 20 mm

diameter (0% Vf)

Like for sample C110, the edge of the core is characterized by the

presence of expansion cracks. As in the periphery than in the centre,

small euhedral crystals are visible (Fig. 20(a)), which attest about the

free space that has existed around them for developing and adopting

their crystalline shape. The size of portlandite crystals ranges from 2

to 5 m (Fig. 20(b)).

86

The puck taken from the sample is very dense. It is cut in the core

using an instrument that has left its mark: the wall of the core is regular

and detached without tearing (Fig. 21 sample C120). Anhedral grains

are joined and the porosity is low (Fig. 21(a)). The grain size is about

1 m (Fig. 21(b)).

4.4. Comparisons and analysis of observations

At a low magnication (Fig. 22), two samples show common features (the expansion cracks): C110 (Fig. 19(a) and C115 (Fig. 22(b)).

The unconned NC1 sample (Fig. 22(a)) is in powder form while C120

appears to be more massive (Fig. 22(c)).

At a higher magnication (1000 to 3000 ), even if NC1

(Fig. 18(b)), C110 (Fig. 19(b)), C115 (Fig. 20(b)) samples are similar

(a) NC1

in grain size, this is not the case with regard to their crystallinity: only

C110 and C115 are characterized by the presence of euhedral crystals

(Fig. 23). Grain size is ner for sample type C120.

The scanning electron microscopy allowed observing the structures

of lime processed under various conditions of connement, both on site

and in the laboratory. The comparison of samples generated in the laboratory shows the difference between unconned and conned, and, for

conned samples, the evolution of structures versus rates of expansion.

Structure and porosity may be compared with the densities of cylinders

(Table 6).

5. Conclusions

A simple model based on the theory of elasticity, on duly validated

experimental data and on reasonable engineering judgement has been

(b) C115

(c) C120

Fig. 22. Comparison of the samples under ESEM (low magnication).

(a) NC1

(b) C110

(c) C115

(d) C120

87

nodules from quicklime on the mechanical characteristics of structural

concrete and on the risk of occurrence of pop-outs likely to inuence

concrete durability. By exploiting this simple model, the following

conclusions can be drawn:

for the range of parameters that have been selected, the pressure

developed at the interface between the concrete and the hydrated

nodule varies from 6 to 60 MPa. The most probable value is of the

order of 20 MPa;

the area of inuence of a nodule is of the order of 2 to 3 times its

diameter;

no local crushing of concrete in the vicinity of a nodule is to be considered. If such a crushing would anyway occur, it would only affect a

very limited zone around the nodule with no impact on the overall

mechanical properties of the concrete;

a micro-cracked zone is likely to develop around the nodule under the

conjunction of unfavourable conditions. The diameter of this cracked

region could be at most of the order of 230% of the diameter of the

nodule and its impact on the strength of the concrete at the macroscopic level is proven as negligible;

for the most probable values of the swelling pressure, the minimum

concrete cover thickness allowing the prevention of the pop-out

phenomenon is of the order of half the diameter of the inclusion. In

other words, under the assumptions considered in this study, no

nodule located at a depth of more than half its diameter should

cause pop-out even when hydrated;

The following conclusions can be drawn from the experimental

programme:

hydration of quicklime in a conned environment, leads to the

production of completely hydrated portlandite nodules;

hydrate formed in a conned environment occupies the available volume and, in present cases, may reach very high densities (average

value = 1.55 g/cm3);

the rate of volume expansion of the quicklime, depending on the free

volume, is very low (average 23% expansion) compared to an

unconned and is the result of a non-full connement;

88

trapped in a concrete structure), the density of the hydrate may

reach up to 1.84 g/cm3, which is still under 2.24 g/cm3 (absolute

and therefore maximum density);

pop-out appears in the test conditions for depths less than or equal to

0.5 times the initial diameter of the nodule of lime;

no internal cracking is observed in the concrete blocks;

when connement is maximal, anhedral grains are joined and the

porosity is low; however, when space around nodules was available,

porosity is large and grain shape is euhedral.

Finally, laboratory tests clearly show that the depth of connement

is the most important factor for explaining pop-out and free lime expansion. Moreover, just the near-to-surface layer is affected by the risk of

pop-out: when the nodule is under the concrete surface, the

surrounding concrete is sufciently resistant to conne the nodule

and avoid explosion.

Under the worst case scenarios in combined terms of swelling

pressure and concrete strength, the minimum thickness necessary to

prevent the pop-out phenomenon is of the order of two times the

diameter of the inclusion. In other words, even under these extremely

unfavourable assumptions, no nodule located at a depth of more than

2 times its diameter should cause pop-outs.

Synopsis

Pop-out induced by lime expansion is a well-known phenomenon.

The concrete cover thickness, the diameter and the shape of the lime

nodule as well as the mechanical characteristics of concrete and lime

are the key parameters inuencing the development of internal pressure and hence controlling the risk of cracking or pop-out. Laboratory

investigations and modelling have been performed and show that the

minimum concrete cover thickness necessary to avoid the development

of the pop-out phenomenon is estimated in the order of half the diameter of the inclusion.

References

[1] C. Plinius Secundus (maior), Natural history, translation from Latin by E. Littr (2nd

Tome), Paris, 1850.

[2] Ph. Dumont, Use of lime in construction, CERES 99/1, University of Lige, Belgium,

1999. (in French).

[3] J.A.H. Oates, Lime and limestone, Chemistry and technology. Production and uses,

Wiley-VCH verlag GmbH, Weiheim, 1998.

[4] R.S. Boynton, Chemistry and Technology of Lime and Limestone, 2nd edition, Wiley

& Sons, New York, (578 pages).

[5] S. Chatterji, Mechanism of expansion of concrete due to the presence of dead burnt

CaO and MgO, Cem. Concr. Res. 25 (1) (1995) 5156.

[6] M.H. Lee, J.C. Lee, Study on the cause of pop-out defects on the concrete wall and

repair method, Constr. Build. Mater. 23 (1) (2009) 482490.

[7] G.M. Idorn, Expansive mechanisms in concrete, Cem. Concr. Res. 22 (1992)

10391046.

[8] A. Verhasselt, Industrial by-products for the design of bonded layers in foundations:

blast furnace slags, iron slags and y ashes, Belgian Road Research Center

Publication, CR 33/91, 1991. (in French).

[9] F. Choquet, Laboratory study for the valorization of iron slags and blast furnace slags

in road engineering, Belgian Road Research Center Publication, CR 22/84, 1984.

(in French).

[10] M. Deng, D. Hong, X. Lan, M. Tang, Mechanism of expansion in hardened cement

pastes with hard-burnt free lime, Cem. Concr. Res. 25 (2) (1995) 440448.

[11] L. Mun-Hwan, L. Jong-Chan, Study on the cause of pop-out defects on concrete wall

and repair method, Constr. Build. Mater. 23 (1) (2009) 482490.

[12] B. Chiaia, A. Fantilli, G. Ferro, G. Ventura, Modeling the CaO hydration in expansive

concrete, in: Bicanic (Ed.), Computational Modelling of Concrete Structures, CRC

Press, 2010, pp. 441449.

[13] H. Shi, L. Yuan, Theoretical and experimental research on expansive stress in

hardened cement paste, Adv. Concr. Res. 4 (2004) 155160.

[14] C.F. Dunant, K.L. Scrivener, Effects of uniaxial stress on alkalisilica reaction induced

expansion of concrete, Cem. Concr. Res. 42 (2012) 567576.

[15] J. Faury, Concrete: inuence of inert components requirements for a better design,

Dunod Ed., Paris, 1942. (in French).

[16] G. Dreux, New guide for concrete, 7th edition Eyrolles Ed., Paris, 1995. (in French).

[17] R.D. Hooton, A.M. Ramezanianpur, R.M. Ahani, U. Schutz, Durability of Portland

limestone cement concrete, International Congress on Durability of Concrete.

ICDC, Trondheim, Norway, 2012. (10 pp.).

[18] B. Chiaia, A. Fantilli, G. Ventura, A chemo-mechanical model of lime hydration in

concrete structures, Constr. Build. Mater. 23 (2012) 308315.

[19] S. Timoshenko, J.N. Goodier, Theory of elasticity, 2nd edition McGraw-Hill Book

Company, 1951.

[20] K. Van Baelen, Carbonation of lime mortars and its effect on historical structures,

(PhD thesis) Catholic University of Leuven (KULeuven), 1991. (in Dutch).

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